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Triethylamine → 5-Chloro-2-isocyanato-1,3-di(propan-2-yl)benzene

HRID 2303587
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HRID 2303587 반응식
[Cl:1][C:2]1[CH:8]=[C:7]([CH:9]([CH3:11])[CH3:10])[C:5]([NH2:6])=[C:4]([CH:12]([CH3:14])[CH3:13])[CH:3]=1.C(N(CC)CC)C.Cl[C:23](Cl)([O:25]C(=O)OC(Cl)(Cl)Cl)Cl>O1CCCC1.CCCCC>[Cl:1][C:2]1[CH:8]=[C:7]([CH:9]([CH3:10])[CH3:11])[C:5]([N:6]=[C:23]=[O:25])=[C:4]([CH:12]([CH3:14])[CH3:13])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 94429TriphosgeneHCID 108891984-Chloro-2,6-diisopropylaniline

생성물 1

HCID 154799605-Chloro-2-isocyanato-1,3-di(propan-2-yl)benzene수율 279%

시약·촉매·용매 2

HCID 8003Pentane용매HCID 8028Tetrahydrofuran용매
2회

실험 절차

To a stirred solution of 4-chloro-2,6-diisopropylaniline (32 grams) and triethylamine-(7.8 mL) in tetrahydrofuran (505 mL) was added triphosgene (14.9 grams). The mixture was refluxed for two hours with stirring. The tetrahydrofuran was then revolved in vacuo and the resulting oil was taken up in pentane and filtered through silica gel to afford 33.3 grams of the product. 1H NMR δ 7.18 (s, 2), 3.22 (qq, 2, J=7.1Hz), 1.25 (d, 6, J=7.1Hz), 1.25 (d, 6, J=7.1 Hz).

후처리

  1. temperatureThe mixture was refluxed for two hours
  2. filtrationfiltered through silica gel

출처 및 근거

ORD 기록
ord-020deb72c4a54b7787f3d7392c80d4f0
출처 데이터셋
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06433009B1

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